Sodium Hydroxide → HCID 14257103, 화합물

HRID 622110

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HRID 622110 반응식
[C:1]([C:6]1[N:10]([CH3:11])[C:9]([S:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)=[N:8][C:7]=1[CH3:22])(OCC)=[O:2].[H-].[Al+3].[H-].[H-].[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl-].[Al+3].[Cl-].[Cl-].[OH-].[Na+]>CCOCC.O>[CH3:11][N:10]1[C:6]([CH2:1][OH:2])=[C:7]([CH3:22])[N:8]=[C:9]1[S:12][CH2:13][C:14]1[CH:15]=[CH:16][C:17]([O:20][CH3:21])=[CH:18][CH:19]=1

참가 물질

8

반응물 5

HCID 14798Sodium HydroxideHCID 6451240Aluminum(III) ChlorideHCID 14257102HCID 14257102, 화합물HCID 21226445Aluminium lithium hydrideHCID 21584524Aluminiumhydride2회

생성물 1

HCID 14257103HCID 14257103, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 3283Diethyl Ether용매4회

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온도
0 °C

실험 절차

5-Carbethoxy-1,4-dimethyl-2-(4-methoxybenzylthio)imidazole (31 g, 0.1 mole) dissolved in ether (250 ml) was added dropwise to a solution of aluminum hydride in ether stirred at 0° C. [the aluminum hydride in ether was prepared by adding lithium aluminum hydride (7.4 g, 0.19 mole) in portions to a solution of aluminum chloride (8.6 g, 0.065 mole) stirred in ether (200 ml) at 0° C⟧ The mixture was stirred at 0° C. for 1 hour, treated with water and 10% aqueous sodium hydroxide, filtered and concentrated in vacuo. The resulting oil was dissolved in methylene chloride, dried with magnesium sulfate, filtered and concentrated in vacuo to give 1,4-dimethyl-5-hydroxymethyl-2-(4-methoxybenzylthio)imidazole.

후처리

  1. customwas prepared
  2. filtrationfiltered
  3. concentrationconcentrated in vacuo
  4. dissolutionThe resulting oil was dissolved in methylene chloride
  5. dry with materialdried with magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-6a7dc7cd8ded4a3c9867fe85a2edfb94
출처 데이터셋
uspto-grants-1988_09
특허 번호
US04769386

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